Gelled mineral oil compositions



United States Patent "ice ABSTRACT OF THE DISCLOSURE Gelled mineral oilcompositions are prepared by blendmg together mineral oil, across-linked polymer of acrylic acid, an aliphatic amine to neutralizethe acrylic acid polymer, and a long chain alcohol. Dyes, pigments,perfumes and the like may be added to the gelled mineral oilcompositions which are useful, for example, in printing lIlkS, cosmeticsand metal protecting formulations.

This application is a continuation-in-part of my copending application,Ser. No. 372,681, filed June 4, 1964 and now abandoned.

This invention relates to gelled mineral oil compositions and to themethod by which they are produced. More particularly, the presentinvention is concerned with a gel comprised of a mineral oil, acrosslinked polymer of acrylic acid, an aliphatic amine neutralizingagent for said polymer, an alcohol having a long carbon chain, and ashort chain alcohol.

Many industrial uses are known for gelled mineral oils, for example, inprinting inks, cosmetics, pharmaceuticals, lubricants, and in metalprotecting formulations. Heretofore, no operable recipe for preparingreproducible mineral oil gels using synthetic polymeric carboxylicthickeners has been devised. It is, therefore, the object of thisinvention to provide a smooth, transparent, homogeneous, stable mineraloil gel.

The composition of this invention is a gel derived from a unique mixturecomprising, as essential ingredients, (A) 100 parts by weight of mineraloil, (B) from 1 to 10 parts by weight of a lightly crosslinkedinterpolymer of an alpha,beta-monoolefinically terminally unsaturatedmonocarboxylic acid having from 3 to 4 carbon atoms (i.e., acrylic andmethacrylic acid) and a polyunsaturated compound copolymerizable withsaid acid and which has at least two alkenyl groups, (C) an aliphaticamine containing a carbon chain having at least 8 carbon atoms, in anamount which is at least sufficient to substantially neutralize theaforesaid acidic interpolymer,

(D) from about to about 100 parts by weight of a saturated aliphaticalcohol having from one to two carbon atoms, i.e., methanol or ethanolor mixtures thereof, referred to herein as the short chain alcohol, and(E) from about 5 to about 100 parts by weight of at least one aliphaticalcohol having from 4 to 22 carbon atoms in the chain, referred toherein as the long chain alcohol.

The several components comprising the gel are blended using aconventional mixing apparatus having a mixing chamber equipped with alow or medium shear agitator. The acrylic acid polymer, a fine powderymaterial, is uniformly dispersed in the mineral oil, the neutralizingamine is then admixed therewith, followed by the addition of the longchain alcohol. The gel is formed when the short chain alcohol is addedto said mixture. The

3,391,081 Patented July 2, 1968 gels preferably are prepared inaccordance with this invention at room temperature, although the ease ofmixing may be facilitated by blending at elevated temperatures sinceviscosity of the blend decreases with increasing temperature; however,care must be taken when compounding at higher temperatures to preventthe loss of the volatile alcohol constituents from the mixing vessel.

In addition to the aforesaid essential constituents of the mineral oilgel, which constituents are defined with greater particularityhereinbelow, various other materials may be incorporated therein to givedesired characteristics and properties to the product. For example,perfumes can be added to mask the unpleasant odors of the long chainalcohols and amines and to impart a pleasant scent to the gel. Dyes orpigments may be easily incorporated therein to provide colored gels.

The mineral oils comprising the base substance of the compositions ofthis invention are the oily liquids obtained by the distillation of thatportion of petroleum which boils between about 330 C. and about 390 C.,and, generally speaking are hydrocarbon oils which are insoluble inwater, alcohol and glycerine and are soluble in ether, chloroform andbenzene. The aforesaid petroleum distillate fraction can be subjected toa purification treatment with sulfuric acid and caustic soda, followedby filtration through decolorizing carbon and cooling and removal ofcrystallized waxes (solid parafiins) to provide the refined mineral oils(also known as liquid petrolatums) which are colorless, tasteless andnearly odorless. Liquid petrolatums may be further classified under thedesignations: light liquid petrolatum having a specific gravity of 0.828to 0.860 and a viscosity range at 100 F. of about to 110 S.U.S.; andheavy liquid petrolatum with a specific gravity of 0.860 to 0.905 and aviscosity range at F. of about 230 to 280 S.U.S. Representative,commercially available mineral oils are sold under the trademarks Nujol,Fractol, Kaydol, Drakeol, Saxol, Alboline, Kremol, Marcol, Wyrol andmany others.

The synthetic resins used as the thickening agents in the gels embodiedherein are the lightly crosslinked interpolymers of acrylic ormethacrylic acid, or mixtures of said acids, with a polyunsaturatedcompound having a plurality of terminally unsaturated polymerizablegroups. Said polymeric thickeners are hereinafter sometimes referred toas acrylic acid polymers or acrylic acid interpolymers for purposes ofbrevity. They are copolymers of said acrylic acids with a minor amount,e.g., about 0.5 to about 2.5% by weight, preferably 0.5 to 2.0% byweight, of the polyunsaturated crosslinking monomer, said percent basedon the Weight of the copolymer. The copolymerization of the monomersor=dinarily is carried out in an inert hydrocarbon diluent using afree-radical catalyst. The crosslinked acrylic acid polymers arerecovered from the polymerization media as white powders. They are highmolecular weight resins, e.g., generally having a molecular weightgreater than about 200,000, preferably greater than about 2,000,000 andusually in the range of about 3,000,000. Such acrylic acid polymers andtheir sodium, ammonium and amine salts are characterized by beinginsoluble in water and in aliphatic and aromatic hydrocarbons; however,they are water-swellable and a small amount thereof can thicken waterinto a heavy mucilage or gel; moreover, the copolymers and their saltsare solvent-sensitive and can thicken non-polar solvents under certainconditions,

but with comparatively less ctfectiveness than in the thickening ofwater. The mineral oil gels embodied herein are characterized by beingsubstantially free of water since mineral oil and Water are generallyincompatible.

Representative polyunsaturated compounds which may be copolymerized withacrylic or methacrylic acid in minor amounts to provide the lightlycrosslinked acrylic acid polymers are the vinyl, allyl and methallylethers of polyhydric alcohols having at least four carbon atoms and atleast three alcoholic hydroxyl groups. The p eferred polyalkenylpolyether monomers are polyallyl sucrose and polyallyl pentaerythritol,desirably containing an average of at least 3 allyl groups for eachmolecule of sucrose or pentaerythritol, the allyl groups attachedthereto by means of ether linkages. The preferred polyallyl sucrosecontains an average of 5 to 6 allyl groups per molecule of sucrose(theoretical maximum is 8 allyl groups) and the preferred polyallylpentaerythritol contains 4 allyl ether groups per molecule {thetheoretical maximum). Acrylic acid copolymers employing erosslinkingmonomers of the aforesaid type are described in US. Patent No.2,798,053. Other polyunsaturated compounds that can be employed toprepare the acrylic acid copolymer additives are the polymericbenzene-soluble products resulting from Na or K polymerization ofdiolefins, preferably conjugated dienes. These polymers have a verylarge proportion of 1.2 structure in the chain and consequently have aplurality of CH side groups which can be copolymerized with the acrylicacids. Acrylic acid interpolymers containing this type of crosslinkingagent are described in US. Patent 2,858,281. Other crosslinking agentsthat can be copolymerized with acrylic and methacrylic acid are thepolyallyl or polymethallyl trimethylene trisulfones. These monomers aredescribed in US. Patents 2,535,533 and 2,535,534 and the acrylic acidcopolymers are described in U.S. Patent 2,958,679. Still othercrosslinking agents that can be employed in producing the acrylic acidcopolymers are the polyvinyl, poly allyl or polymethallyl silanes or thecorresponding tin compounds. In these compounds the silicon or tin atomis connected to a carbon atom by a covalent bond. The silicon or tincompound, of course, must have at least two of the unsaturated groupsmentioned above. Particularly good crosslinked polymers can be preparedby copolymerizing tetrallyl or tetravinyl silane or tin with the acrylicacids. However, satisfactory copolymers can be produced with tincompounds having two or three of the groups, vinyl, allyl or methallyl.The remainder of the silicon or tin atom can have any nontoxic group andparticularly an alkyl group. The acrylic acid eopolymers made with thepolyallyl or polyvinylsilane or tin compounds are described in US.Patent 2,985,631. Still another crosslinked acrylic acid polymersuitable as a thickener for the gels of this invention are thecopolymers of acrylic or methacrylic acid with small amounts of apolyallyl phosphate ester as the crOsslinking agent, said copolymersbeing described in the copending U.S. Patent application of Frank A.Wagner, Ser. No. 425.338 filed Jan. 13, 1965. The allyl phosphatesembodied therein conform to the formula R r B OIIz=(J-CIIz-O-l-OCII2--C=ti7Ila atom, an allyl radical, a methallyl radical,an alkyl radical, i

an aralkyl radical, an aryl radical and an alkaryl radical. From thisclass of monomers triallyl phosphate is pre fe-rred.

The mixtures of this invention contain at least about one part ofcrosslinked acrylic acid polymer per l parts by weight of mineral oiland no practical advantage in increased thickening is gained by usingmore than about 10 parts of the resin per 100 parts of mineral oil. Thepreferred range is from about 3 to parts of polymer per 100 parts ofoil.

The acrylic acid polymer is uniformly dispersed in the oil and thenconverted to an amine salt by adding to the mixture a saturated orunsaturated aliphatic amine, or mixtures of said aliphatic amines, saidamine containing at least one carbon chain having at least 8 carbonatoms attached to the amine nitrogen atom. Preferred, however, arecarbon chains having from to 22 carbon atoms. Suitable amineneutralizing agents thus include the higher aliphatic primary, secondaryand tertiary amines derived from fatty acids and mixtures thereof (i.e.,the fatty amines). A comprehensive survey of fatty acids from which suchamines are derived is found in the Encyclopedia of Chemical Technologyby Kirk and Othrner, John Wiley and Sons, Inc., New York, N.Y., volume 6(1951), pp. l73-178. Fatty amines are described in detail on pp. l27l35of the Encyclopedia of Chemical Technology," Second Edition, volume 2(1963). Representative amines are the octyl, dodecyl, tetradecyl,hexadecyl, octadecyl, arachic, lauroleic, myristoleic, palmitoleic,oleic, erucic, linoleic, eleostearic, linolenic, didodecyl.ditetradecyl, dioctadecyl, dicoco, di(octadecenylbctadecadienyl),trioctyl, tridodeeyl, and tricoco amines and the like and mixturesthereof. Most preferred herein are the primary, secondary and tertiaryamines possessing one or more aliphatic chains having from 12 to 18carbon atoms and mixtures thereof.

The amine is admixed with the oil and resin in an amount which is atleast sufiicient to substantially neutralize the acrylic acid polymer.This amount is easily determined by simple calculations involving theequivalent weights thereof. However, it has been found that the use ofexcess amine, for example, from about 2 to about 5 times that requiredto neutralize the acrylic acid polymer, results in clearer, higherviscosity gels. The preferred ratio is about 2 to 3 equivalents of amineper equivalent of acrylic acid polymer.

The compositions prepared according to this invention contain, per 100parts by weight of mineral oil, from about 5 to about 100 parts,preferably from about 5 to about 20 parts, of a lower aliphatic,saturated alcohol selected from the group consisting of methanol,ethanol and mixtures thereof. It has been found that the compositionsmust also contain in admixture one or more long chain aliphaticalcohols, that is, alcohols which have at least 4 carbon atoms. Althoughalcohols containing up to 22 carbon atoms are operable, those having 8to 18 carbon atoms are preferred. The amount of long chain alcoholrequired in the blends ranges from about 5 to about 100 parts, andpreferably from about 10 to about parts, based on parts of mineral oil.Representative alcohols in the so-called long-chain alcohol categoryreferred to herein are the saturated primary, secondary and tertiaryalcohols having at least 4 carbon atoms such as the butanols, the amylalcohols, the hexanols, the heptanols, the oetanols, nonyl alcohol,decanol, dodecanol. tetradecanol, cetyl alcohol, octadecanol, and thelike and mixtures thereof; and the ethylenically unsaturated alcoholshaving at least 4 carbon atoms and from one to three olefinic bonds inthe carbon chain, such as lauroleyl alcohol, myristoleyl alcohol,palmitoleyl alcohol, oleyl alcohol, erucyl alcohol, linoleyl alcohol,linoleneyl alcohol, and the like and mixtures therepf.

Smooth, homogeneous and stable mineral oil gels will not be obtainedunless the aforedescribed multi-alcohol system is utilized incompounding the blends. By the term stable gel is meant one which willnot separate into layers of the several components incorporated thereinimmediately or even after long storage periods. The gels preparedaccording to this invention are stable for at least six months andfrequently for an indefinite period. Homogenous gels can be preparedwithin a wide range of viscosities, ranging from thin pourable gels witha viscosity of about 100 centipoise at 25 C. to thick rubbery gelsArmeen 12D: a mixture of fatty amines derived from a mixture of fattyacids having to 14 carbon atoms.

Armeen 18D: a mixture of fatty amines derived from a mixture of fattyacids having 16 to 18 carbon atoms. The

of greater than 200,000 centipoise viscosity. The viscosity 5 Armeenfatty acid amines, sold by Armour and Co., of the gel product is afunction of the amount of acrylic Chicago, Illinois, are described onpage 62 of the Handacid polymer used, the amount and type of amine, andbook of Material Trade Names by Zimmerman and Lathe long chain alcoholused. In general, the longer the vine, Industrial Research Service,Dover, N.H., (1953). Carbon Chain f the amine used as the neutralizingagent, The mixtures described in the examples set forth hereinthe higherthe Viscosity of the resulting 10 below were prepared at roomtemperature in the following EXAMPLES manner. The powdery acrylic acidpolymer was dispersed in the mineral oil using an air driven propellerstirrer. The

In the llmstratlvefmkfodments Set forth herelnbtaflow neutralizing aminewas then slowly added with continuous the following materials identifiedby trademark designamining followed by a rapid addition of the longchain were employed; alcohol. The short chain alcohol was then addedthereto Mmeral 0115 and the mixture was given a short period ofagitation. If

Kaydol L-l and Kaydol L16: clear, white, rethe composition met therequirements of this invention, fined liquid petrolatum having an A.P.I.gravity of 27.4 there was a viscosity increase and subsequent gelformato 29.3 and a Saybolt Viscosity at 100 C. of 345 to 355. tion.Viscosity of the products was measured at C. The Kaydol mineral oils aresold by L. Sonneborn 0 using a Brookfield Model RVT Viscometer. Amountsof s In Chica Illingis, ingredients specified in the examples are givenin parts by Drakeol 19: a refined, clear liquid petrolatum havweight. ina specific gravity of 0.864 to 0.873 at 77 F., and a EXAMPLE 1 viscosityof 185 SSU at 100 F. and 44.5 SSU at 210 F.

Drakeol 35: a refined, colorless liquid petrolatum 25 In thls Series ofexperlments m zed m T ble A having a specific gravity of 0.875 to 0.883at 77 F, and l VarlOuS formulations not e nf 9 the a viscosity f 360 SSUat 100 F d 54 SSU at 210 R quirements for mixtures within the scope ofthe invention The Drakeol mineral Oils are 501 d by the PennSy1 (1.e., wth regard to the alcohol components) failed to g ive the desiredhomogeneous mineral oll gel. When a cond1t1on Vania Refining Company,Butler, Pennsylvania. d h f 1 Rocket H and Certrex 56: tan-colored,partiallyof No Ge 15 reporte mt e.sum.mary 0 resu F was fi d ineral Oilssold b the Socony M Ob on usually observed that the acrylic acid polymerprecipitated i y from the mixture of oil and alcohols as a rubbery mass,

or in a few cases there was no appreciable thickening of Acryhc andcopolymers the blend. When the alcohol component consisted solelyCopolymer A: copolymer of acrylic acid and about of methanol, ethanol orisopropanol, no gel was formed y Weight of a polyallyl ether of Sucroseng an or there was a light gel which separated into layers; the av ag ofabout allyl groups P each Sucrose ol use of a sole alcohol containing 4or 5 carbon atoms recule. sulted in merely a slightly thickened mixtureor a light Copolymer B: a copolymer of acrylic acid and ab t non-uniformgel. Various combinations of alcohols which 1% by weight of thepolyallyl ether of pentael'ythritol 40 were not in accordance with therequirements of this in- (tetraallyl pentaerythritol). vention also gaveunsatisfactory results as shown in the Copolymer C: a copolymer ofacrylic acid and ap table.'

TABLE A Composition of Mixture Ratio of E Acrylic Acid Amine 2Equivalents of Viscosity of Gel in No. Mineral Oil Polymer 1 (ArmeenAmine to Alcohol (parts) Alcohol (parts) ecntipolses and Remarks (100parts) (copolymer CD), parts Equivalents of A), parts Acrylic AcidPolymer- 1 Kaydol L-1" 4.3 8.6 0.7/1 Methanol (10) No Gel. d 5 20 1.5/1..do Do. 5 15 1.1/1 Methanol Do. 5 15 1.1/1 Methanol (100) Do. 5 30 2.3/1 Methanol (10) Do. 5 45 3. 4/1 do Do. 5 4.1/1 (lo Do. 5 20 1. 5/1Ethanol (30) 4,200; separation of components. 5 20 1.5/1 Ethanol (l0)Isopropanol (20) 7,500; separation of components. 5 20 1. 5/1Isopropanol (18). Gel. 5 20 1.5/1 Isopropanol (10). Isooctano 20) Do. 520 1. 5/1 n-Butauol (20)... 10,000; separation oi components. 5 20 1.5/1Ethanol (l0) Isopropanol (20) 6,250; separation of components. 5 20 1.5/1 Amyl alcohol (20) 575. 5 20 1. 5/1 Ethanol (l0) Allyl alcohol (20)9,770; separation of components.

Equivalent weight of about 75.

proximately 0.5% by weight of the polyallyl ether of pentaerythritol.

Neutralizing amines Armeen CD: a mixture of fatty amines having amolecular combining weight (equivalent weight) within the range of about185 to 206, derived from coconut oil fatty acids (a mixture of fattyacids having from 8 to 18 carbon atoms).

2 Equivalent weight of about 185 to 206.

EXAMPLE II iABLE B om posi tion of Mixture Viscosity of Ex. .lcrylieAcid Polymer, 5 .l'lnnnc 1 Ratio of Equiv- Alcohol. parts ox- N 0.Mineral oil, 100 parts except where otherl.-\rmeen \ilent Amine cert-twhere other- Alcohol (parts) Ceniipoiscs parts wise indicated 131).parts to Equivalent W150 indicated Polymer 16 Kaydol L-1... Copolymer A,3 parts 2/1 13,000 17.. do ...do 0.4/1 34,000 110.. It. 5/1 114, 000 t.5/1 52, 000 ..d0. 11.5/1 102,000 olymer B t). 5/1 3 450 t/l 49,000 11/182,000 5/1 124,000 12/1 116,000 13/1 120, 000 .00-. .3 in 114,000Ccpolyme 1 .30 1.5/1 57,000 110.... .10 1.5/1 78,000 it) 1.511 131,000 2t 13, 600 10 o 74, 000 ..do J0 Iso-octanol (40).. 110,000 Copolymer A..10 Ethanol n-Butanol 28,250 ....tio .....do Iso-butanol (20 28,000 .10.110 Amyl alcohol (20) 59,000 L0 Octanel (20) 88, 000 30 Deconol (20)100,000

20 Duodecanol (20). .0 i nButan0l (20).. 44, 600 .30 It. Iso-butanol(20) 48,000 .10 i. Amyl alcohol (20) 55,000 I Iso-amyl alcohol (20)55,000 .10 l. Hexanol (20) 68, 400 .20 1.5 Heptanol (20). 82,000 .10 ll.5/1 Octanol (20)... 88,000 ."0 t. 5/1 Iso-octanol (20) 95,000 110 1. 5/1Decanol (20).... 105,000 .10 1. 5/1 Duodeeanol (20). 132,000 .10 t. 5/1Iso-octanol 44,000 .10 1. 5/1 Iso-oetanol (20)... 61,000 to l1Isa-octanol (40) 115,000 lit) .do 77, 000 .U ..do- 110,000 .10 1.5/1 do-200, 000 110 1. 5/1 .(10 113, 000

methanol (10).

i 30 Ii.0/1 Methanol Iso-octanol (20) 200, 000 24. 5 t. 9/1 do- .do 04,000 116 II/I o ..d0 200,000

1 Equivalent weight of about 75.

2 Equivalent weight of about 185 to 206. 3 N0 gel (insuilicient amine).

4 Very thick gel, viscosity not measured.

EXAMPLE III The tests set forth in this example illustrate theepecificity of the type of amine neutralizing agent suitable for thecompositions of this invention. The mixtures consisted of 100 parts ofKaydol L-l mineral oil, 5 parts of Copolymer B acrylic acid polymer, thespecified amine in an amount such that the ratio of equivalent of amineto equivalent of acrylic acid polymer was about 2 to 1, 20 parts ofiso-octanol and 10 parts of methanol. The data are presented in Table C.No satisfactory homogeneous gel was formed with any of the mixtures ofthis example. Either the acrylic acid polymeramine salt precipitatedfrom the mixture of oil and alcohols as a rubbery mass, or the polymerwas seen as a fioccuiated mass, or there Was formed a light gel whichseparated into layers.

TABLE C Ex. N o. Amine Characteristics of Mixture Mixed isopropanolamine Precipitation. 61.. Diethanolamine Flocculation. 62Triethanolamine. Precipitation. 63-- Dibutyl amine Do. 04.-Bis(1ethy1,3-methylpentyl)arnine Do. 65.. Dicyclohexyl amineFlocculation. 60.- 2(2arnino ethoxy ethanol amine Precipitation. 67.-Di-Z-ethyl hexyl amine- Do. 08.- Benz l amine D0. 09 N-aminoethylpipcrazine-. Separation.

It is to be understood that the foregoing examples of specificembodiments of the invention are merely illustrative and not limitingsince modifications and variations may be made without departing fromthe scope and spirit of the invention as defined by the appended claims.Stated dillercntly, the essence of invention toit .Armeen 18D Armeen12D" 1 Oleylamine.

sides in the formation of a gelled mineral oil composition comprising ablend of mineral oil with an amineneutralized, crosslinked acrylic acidpolymer, and a plurality of alcohols. The addition of other materialsand substances to the composition to provide diverse desirableproperties and characteristics thereto is of course contemplated to bewithin the ambit of the invention.

I claim:

1. A gelled mineral oil composition comprising a mixture of (A) parts byweight of mineral oil,

(B) from about 1 to about 10 parts by weight of a crosslinkedinterpolymer of an alpha, beta-monoolefinically terminally unsaturatedmonocarboxylic acid having from 3 to 4 carbon atoms and apolyunsaturated compound selected from the group consisting of ethcrs,hydrocarbons, sulfones, silanes and corresponding tin compounds, andphosphates having at least two alkenyl groups and copolymerizable withsaid acid,

(C) an aliphatic amine having at least one carbon chain containing atleast 8 carbon atoms attached to the amine nitrogen atom, said aminepresent in an amount which is at least sufiicient to substantiallyneutralize the aforesaid acidic interpolymer,

(D) from about 5 to about 100 parts by weight of aliphatic alcoholhaving from 4 to 22 carbon atoms, and

{15) from about 5 to about 100 parts by weight of an alcohol selectedfrom the group consisting of methanol, ethanol and mixtures thereof.

2. The gelled mineral oil composition of claim 1.

wherein (C) is an amine selected from the group consisting of aliphaticprimary, secondary and tertiary amines and mixtures thereof, having acarbon chain attached to the amine nitrogen atom containing from 8 to 22carbon atoms, said amine present in an amount which is at leastsufficient to substantially neutralize the aforesaid interpolymer, and

(D) is an aliphatic alcohol having from 8 to 18 carbon atoms.

3. The composition according to claim 2 wherein component (B) is aninterpolymer of acrylic acid and said polyunsaturated compound, andcomponent (C) is from about 1 to about equivalents, per equivalent ofacrylic acid interpolymer, of aliphatic primary amine.

4. The composition according to claim 3 wherein there is from about 3 toabout 5 parts by weight of component (B), from about to about 40 partsof component (D) and from about 5 to about 20 parts of component (E).

5. A gelled mineral oil composition of claim 1 wherein (B) is acrosslinked interpolymer of acrylic acid and about 0.5 to about 2.5%,based on the weight .of the interpolymer, of a polyunsaturated compoundhaving at least two alkenyl groups and copolymerizable with acrylicacid,

(C) is present in amounts from about 2 to about 3 equivalents, perequivalent of the aforesaid acrylic acid interpolymer, and is an amineselected from the group consisting of aliphatic primary, secondary andtertiary amines and mixtures thereof, said amine having a carbon chaincontaining from 8 to 18 carbon atoms attached to the amine nitrogenatom,

(D) is present in amounts of from about 10 to about 40 parts by weightand is an aliphatic alcohol having from 8 to 18 carbon atoms, and

(E) is present in amounts of from about 5 to about 20 parts.

6. The composition according to claim 5 wherein there is from about 3 toabout 5 parts of the interpolymer of acrylic acid and the aliphaticamine is a primary amine.

7. A method of gelling mineral oil which comprises the steps of (a)uniformly dispersing in 100 parts by weight of mineral oil from about 1to about 10 parts by weight of a powdery crosslinked interpolymer of analpha, beta-monoolefinically terminally unsaturated monocarboxylic acidhaving from 3 to 4 carbon atoms and a polyunsaturated compound selectedfrom the group consisting of others, hydrocarbons, sulfones, silanes andcorresponding tin compounds, and phosphates having at least two alkenylgroups and c.opolymerizable with said acid,

(b) mixing therewith an aliphatic amine having at least one carbon chaincontaining at least 8 carbon atoms attached to the amine nitrogen atom,said amine being added in an amount which is at least sufiicient tosubstantially neutralize the aforesaid acidic interpolymer,

(c) mixing therewith from about 5 to about parts by Weight of aliphaticalcohol having from 4 to 22 carbon atoms, and

(d) mixing therewith from about 5 to about 100 parts by weight of analcohol selected from the group consisting of methanol, ethanol andmixtures thereof.

8. The method of claim 7 wherein, in

(a) the crosslinked interpolymer is an interpolymer of acrylic acid andabout 0.5 to about 2.5%, based on the weight of the interpolymer, of apolyunsaturated compound having at least two alkenyl groups andcopolymerizable with acrylic acid,

(b) from about 2 to about 3 equivalents, per equivalent of the aforesaidacrylic acid interpolymer, of amine selected from the group consistingof aliphatic primary, secondary and tertiary amines and mixturesthereof, said amine having a carbon chain containing from 8 to 18 carbonatoms attached to the amine nitrogen atom, and mixed with (a),

(c) there is about 10 to about 40 parts by weight of aliphatic alcoholhaving from 8 to 18 carbon atoms, and in (d) there is about 5 to about20 parts of an alcohol.

References Cited UNITED STATES PATENTS 2,652,363 9/1953 Woods et a1.252-34.7 2,923,692 2/1960 Ackerman et al. 2602.2 3,148,958 9/1964 Monick44-7 3,226,373 12/1965 Fareri 25234 DANIEL E. WYMAN, Primary Examiner.

I. VAUGHN, Assistant Examiner.

